HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethylene Glycol → Ethyl 1,4-dioxaspiro(4.5)decane-8-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethylene Glycol | HCID 174 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Ethyl 4-oxocyclohexanecarboxylate | HCID 317638 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | Ethyl 1,4-dioxaspiro(4.5)decane-8-carboxylate | HCID 10488810 | 74% |
Reaction Steps
A solution of ethyl-4-oxocyclohexane carboxylate (28.9 g, 169 mmol), ethylene glycol (36.7 g, 33.0 mL, 592 mmol) and p-toluol sulphonic acid (380 mg, 2.0 mmol) in toluol (90 mL) was stirred overnight at room temperature. The reaction solution was poured into ether (150 mL) and washed with water and 5% sodium hydrogencarbonate solution (150 mL each). The organic phase was dried with sodium sulphate and concentrated to low volume in a vacuum. Since the raw product (26.8 g) was obtained in pure form, it could be directly converted further.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08835689B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-a50e16590754406da19979d914182275 |
| Source note | uspto-grants-2014_09 |